JIS JAPANESE INDUSTRIAL STANDARD Translated and Published by Japanese Standards Association JIS Z 2371-20 Methods of salt spray testing Ics 77.060 Descriptors : metals, coatings, corrosion tests, salt-spray tests Reference number : JIS Z 2371 : 2000 (E)Z 2371 : 2000 Foreword This translation has been made based on the original Japanese Industrial Standard revised by the Minister of International Trade and Industry through deliberations at the Japanese Industrial Standards Committee in accordance with the Industrial Standardization Law. Consequently JIS Z 2371:1994 is replaced with JIS Z 2371:2000. This revision has been prepared based on ISO 9227:1990 Corrosion tests in artificial atmospheres — Salt spray tests for the purposes of comparison and conformity with the International Standard. Date of Establishment: 1955-12-16 Date of Revision: 2000-02-20 Date of Public Notice in Official Gazette: 2000-02-21 Investigated by: Japanese Industrial Standards Committee Divisional Council on Basic Items JIS Z 2371: 2000, First English edition published in 2000-11 Translated and published by: Japanese Standards Association 4-1-24, Akasaka, Minato-ku, Tokyo, 107-8440 JAPAN In the event of any doubts arising as to the contents, the original JIS is to be the final authority. © JsA 2000 All rights reserved, Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from the publisher. Printed in JapanJAPANESE INDUSTRIAL STANDARD JIS Z 2371: 2000 Methods of salt spray testing Introduction This Japanese Industrial Standard has been prepared based on the first edition of ISO 9227 Corrosion tests in artificial atmospheres — Salt spray tests published in 1990. However, some items and contents not specified in the corresponding International Standard have been added, and some parts have been rejected because the experimental results of the reference specimens specified have not conformed to the requirements. The main differences are shown as follows: The rejected part: The evaluation method for reproducibility of testing apparatus The portions underlined with dots or sidelined in this Standard are the items not specified in the corresponding International Standard. 1 Scope This Japanese Industrial Standard specifies the required apparatus, reagent, technique or acceptance criteria when the corrosion resistance test of metallic materials or of those electroplated or treated with inorganic or organic films by the methods of neutral salt spray test (NSS), acetic acid salt spray test (AASS) or CASS test (CASS). Remarks: The International Standard corresponding to this Standard is listed as follows. ISO 9227: 1990 Corrosion tests in artificial atmospheres — Salt spray tests 2 Normative references The following standards contain provision which, through reference in this Standard, constitute provisions of this Standard, the most recent editions of the standards (including amendments) indicated below shall be applied. JIS G 3141 Cold-reduced carbon steel sheets and strip Remarks: The provisions cited from ISO 3574: 1986 Cold-reduced carbon steel sheet of commercial and drawing qualities are equivalent to the corresponding provisions of the said standard. JIS K 0557 Water used for industrial water and wastewater analysis JIS K 8145 Copper (Il) chloride dihydrate JIS K 8150 Sodium chloride JIS K 8180 Hydrochloric acid JIS K 8355 Acetic acid JIS K 8576 Sodium hydroxide JIS K 8847 Hexamethylenetetramine JIS Z 8802 Methods for determination of pH of aqueous solutions 3 Apparatus The apparatus necessary to salt spray testing shall be composed of an atomizing chamber equipped with an atomizer, a testing salt solution reservoir, a specimen support, atomized solution sampling containers, a temperature controller,2 Z 2371 : 2000 ete; a salt water supply tank, a compressed air feeder, an air saturator, an exhauster, etc., and shall conform to the following requirements: a) The atomizer shall have the performance to spray atomized solution uniformly on a specimen from the upper part (refer to Annex 2). b) The atomizing chamber shall be not less than 0.2 m* in volume. Its shape and dimensions may be optional. ¢) The ceiling or cover of the atomizing chamber shall be so constructed that no drops of solution adhering to its inner surface fall on a specimen. d) Corrosive materials shall not be used for the apparatus. e) The apparatus shall be so constructed that the temperature and atomization in the atomizing chamber are not influenced by the open air and the solution fallen from the specimen is not reused for the testing. f) The specimen support shall be capable of keeping the specimen at a specific angle (). Note () The materials of specimen supports shall be glass, rubber, plastics, or suitably coated wood, and the specimen should preferably be supported from the underside of the bottom or the side face. The specimen may be hung by a glass hook or a vinyl string, provided it is kept in a specific position. If necessary, the specimen is supported from the bottom. g) The atomized solution sampling container shall be a clean container of 100 mm in diameter in sampling surface and 80 cm? in horizontal sampling area, and the containers shall be placed at not less than two positions so as to ensure the uniformity of atomization, for example, near the specimens, and one close to the atomizer and one remote from. h) The exhauster shall not be influenced by the wind pressure of the open air. i) The maintenance and control of the apparatus shall always be correctly carried 4 Specimen The dimensions and shape of the specimen should preferably be a flat sheet of ’ 80. 1.0 |. However, other dimensions or member may be used subject to the agreement between the parties concerned with delivery. Informative reference: For the specimen of different metal possible to be mutually 5 Preparation of specimen The specimen shall be free from stains or flaws. The preparation of the specimen shall be as follows: a) The section of the specimen shall be protected by a stable covering material under test conditions, as required (?). Note (?) The covering material includes a tape, paint, paraffin, etc. b) Metallic and metallic coated specimens shall be suitably cleaned beforehand. Cleaning shall be carried out by an appropriate method according to the nature of surface and the contaminants. Abrasives other than past; ecipitated calcium ini i i ide, or detergents causing a corrosive or protective coating shall not be applied.3 Z.2871 : 2000 ‘The specimen, after cleaning, shall be protected from contamination. c) The specimen coated with paint and non-metallic coatings shall not be, prior to test, subjected to cleaning or other treatments. However, the adhering matter incovenient to test may be removed. Furth ired to 6 Angle and position of specimens during testing The angle and position of the specimens in the atomizing chamber during testing shall conform to the following conditions (refer to Annex 3): a) The angle of the specimens shall be 20° + 5° to the vertical line. In the case of a member, it shall be placed with its significant surface at 20° + 5° to the vertical line. Other angles may be employed subject-to the agreement between the parties concerned with delivery. The surfaces of the specimens shall be exposed to the motion of free atomization, and shall be placed in the atomizing chamber not to intersect the stream of spray from the atomizing nozzle at right angles. b) The specimens shall contact with nothing other than the support. ¢) Each specimen shall be so positioned and spaced as not to interfere with the free falling of the spray. 4) The salt solution dripping from one specimen shall not fall on other specimens. 7 Salt solution for testing 7.1 Preparation method of salt solution for testing The preparation method of salt solution shall be as follows: a) Salt The salt shall be the sodium chloride of special grade specified in JIS K 8150 or equal to or higher grade(*). Note (*) The equal to or higher grade means that copper content shall be less than 0.01 g/kg and nickel content shall be less than 0.01 g/kg when sodium chloride is measured by the means of atomic absorption spectrometry or other analytical method with the same accuracy. Furthermore, the content of sodium iodide shall not exceed 1.0 g/kg or the total amount of impurities as converted to dry salt shall not exceed 5.0 ghkg. b) Water The water shall be the deionized water or distilled water not more than 20 uS/em in electric conductivity at 25 °C + 2 °C.4 Z 2371: 2000 It is recommended that the electric conductivity ought to be not more than 1 uS/em. c) Preparation method Dissolve the salt in a) in the water in b), and adjust the salt concentration to 50 g/l + 5 g/l. As to the adjusted result, measure the density using a hydrometer, and confirm that it is within the range of 1.029 to 1.036 at 25 °C. If it is found to be outside this range, adjust the solution again. 7.2 pH control 7.2.1 Neutral salt spray test The salt solution for testing shall be free from suspended substance(*) before atomization and the atomized solution sampled at spraying shall be within the range of 6.5 to 7.2 in pH(). In regulating pH, 0.1 mol/I solution of the sodium hydroxide specified in JIS K 8576 or hydrochloric acid specified in JIS K 8180 shall be used, as required. The measurement of pH shall be carried out at 25 °C + 2 °C in accordance with JIS Z 8802. In routine checks, the pH may be examined with a pH test paper readable to the place of 0.3. Notes (#) If suspended substance does not disappear by sufficient mixing, the solution filtered through filter paper or the like is used. (©) The following methods can be used in order that the pH of atomized solution sampled, during atomization of salt solution for testing at 35 °C, is within the range of 6.5 to 7.2. a) When the pH of salt solution is regulated at a room temperature and the solution is sprayed at 35 °C, pH of the sampled solution generally becomes higher than that of the original due to the volatilization of carbon dioxide dissolved in the solution. Therefore, when the pH of salt solution is regulated at 25 °C + 2°C, it is kept at about 6.5 level. b) After boiling quietly for about 30 s, the salt solution is cooled to 25 °C, or after keeping at 35 °C for 48 h, the pH is regulated. ¢) Salt solution is prepared by using the water in which carbon dioxide is not contained by heating at 35 °C or higher (Remarks 4 in 4 of JIS K 0557) and then the pH is regulated. 7.2.2 Acetic acid salt spray test The salt solution for testing shall be free from suspended substance(*) before atomization and the acetic acid specified in JIS K 8355 shall be sufficiently added so that the atomized solution sampled at spraying is within the range of 3.1 to 3.3 in pH. The pH of salt solution should be regulated at 3.0 to 3.1 at first for the purpose of making the pH of sampled solution fall under the specified range. The measurement of pH shall be carried out at 25 °C + 2 °C in accordance with JIS Z 8802 and corrected appropriately by adding the acetic acid specified in JIS K 8355 or sodium hydroxide specified in JIS K 8576, as required. In routine checks, the pH may be examined with a pH test paper readable to the place of 0.1.5 Z 2371 : 2000 that.0.1.mol/ 7.2.3 CASS test Add 0.205 g + 0.015 g of copper (II) chloride (0.26 g + 0.02 g of copper (II) chloride dihydrate specified in JIS K 8145) per 1 / of the salt solution for testing. Next, regulate the pH in accordance with the method specified in 7.2.2. 8 Supplied air The compressed air to be supplied to the nozzle for atomizing salt solution shall be free from oil and dust, and its pressure shall be kept at 0.07 MPa to 0.17 MPa. It is recommended that it ought to be kept at 0.098 Mpa + 0.010 MPa. 9 Conditions in atomizing chamber The conditions in atomizing chamber shall be as follows: a) Temperature The temperature around the specimen holder in the atomizing chamber shall be kept at 35 °C + 2 °C for the neutral and acetic acid salt spray test, and at 50 °C + 2 °C for the CASS test. The measuring position of temperature shall be at least 100 mm apart from the wall. b) Temperature and water level of salt solution reservoir for testing The temperature of the salt solution reservoir for testing shall be kept at 35 °C + 2 °C for the neutral and acetic acid salt spray test and at 50 °C + 2 °C for the CASS test. The water level of the salt solution reservoir for testing shall be kept at constant level. c) Spray The sprayed particles shall, as a rule, fall free, and be baffled from impinging directly on a specimen by facing the atomizing nozzle to the direction where the specimen is clear of the direct spray. 4) Atomization sampling solution After an operation of consecutive 24 h under a state where the inside of the atomizing chamber is filled up with specimens of specified dimensions and shape, the sampling amount of atomized solution collected shall average 1.5 ml + 0.5 ml per 1 h for each 80 cm? of horizontal sampling area. In this case, the salt concentration of sampled atomized solution shall be 50 g/l+ 5 g/l. Further its pH shall be 6.5 to 7.2 for the neutral salt spray test and 3.1 to 3.3 for the acetic acid salt spray test and CASS test. The measurement of pH shall be carried out in accordance with the method specified in 7.2. Informative reference: If the density is in the range of 1.029 to 1.036 at 25 °C when measured using a hydrometer in the case of the neutral salt spray test, the salt concentration of atomizing solution is considered to conform to the specified requirements. 10 Reuse of apparatus When the apparatus has been used for the spray test with a different salt solution for testing or for other purpose, the apparatus shall be cleaned before use. When the test is started again, the apparatus shall be operated at least for 24 h before the specimen is placed in the chamber and it shall be verified that the pH of sampled solution is within the specified value throughout the entire spraying period.6 22371 : 2000 11 Evaluation method of reproducibility of testing apparatus In order to verify the reproducibility of test results by one set of testing apparatus or by the same type of apparatus in different laboratories, the apparatus shall be required to verify the motions periodically in accordance with 11.1 to 11.3. 11.1 Neutral salt spray test 11.1.1 Reference specimens In order to verify the motions of apparatus, use four pieces of the reference specimens of Grade SPCE steel sheets specified in JIS G 3141 of which the dimensions are 70 mm x 150 mm and 1 mm + 0.2 mm in thickness and the surface is free from defects [roughness (arithmetic mean) deviation: R,=0.8 +0.3 um, the value along the rolling direction]. These reference specimens shall be taken by cutting from cold-rolled steel sheets. ‘The reference specimens shall be carefully cleaned immediately before testing. The dirt, oil and other impurities capable of influencing the test results shall be removed by cleaning. In such a case, either of the following methods shall be used. a) Thoroughly clean the reference specimens with an appropriate organic solvent (the range of boiling point of hydrocarbon, 60 °C to 120 °C) using a clean, soft brush or an ultrasonic cleaning device. Carry out the cleaning in a vessel full of solvent at room temperature. After cleaning, rinse the reference specimens with fresh solvent and then dry them. b) If the similar results are obtained, other methods may be used in accordance with the agreement between the parties concerned with delivery. Weigh the reference specimens to the place of 1 mg. Protect the one surface of the reference specimens with a removable coating material, for example, an adhesive tape. 11.1.2 Arrangement of the reference specimens Position the four reference specimens in four different corners in the test chamber, with the unprotected surface upwards, and at an angle of 20° + 5°. The support for the reference specimens shall be made of, or coated with, inert materials such as plastics. The lower edge of the reference specimens shall be approximately level with the upper edge of the salt spray collector so as to be exposed as the same manner as the ordinary plane specimens. The test duration shall be 96 h. 11.1.3 Determination of decrement At the end of test, remove the coating material, rinse the reference specimens with cold water and remove the salt deposit. Immerse the reference specimens in the cleaning solution prepared by the method in which 3.5 g of the hexamethylenetetramine specified in JIS K 8847 is added as a corrosion inhibitor in 1 / of the solution [50 % (v/v)] prepared so that 1 volume of the water in 7.1 b) is added in 1 volume of the hydrochloric acid specified in JIS K 8180, repeat the cleaning until the decrement change almost disappears and remove the corrosion products thoroughly. It is recommended that the temperature of cleaning solution ought to be 25 °C + 2 °C. After removing, clean the reference specimens thoroughly with water at ordinary temperature and dry them at the end. Remarks: In order to clean sufficiently with water, it is recommended that the floating matter on the surface ought to be washed out with service water.7 Z 2371 : 2000 Weigh the reference specimens to the place of 1 mg and calculate the decrement of mass by the unit of g/m?. 11.1.4 Inspection of apparatus operation If the mass loss of each reference specimen at four positions is 140 g/m*30 g/m®, the apparatus shall be considered to operate satisfactorily. Remarks: Zine plate may be used in place of steel plate. In such a case, the dimensions of specimen, cleaning method and measuring method of decrement shall be in accordance with 11.2, and if the mass loss is 50 g/m? + 15 g/m?, the apparatus shall be considered to operate satisfactorily. 11.2 Acetic acid salt spray test 11.2.1 Reference specimens In order to verify the motions of apparatus, use four pieces of the reference specimens of zinc plate conforming to the chemical composition given in Table 1 and of which the dimensions are 70 mm x 150 mm and 1 mm + 0.2 mm in thickness and the surface is free from defects [roughness (arithmetic mean) deviation: R= 0.05 um + 0.02 um, the value along the rolling direction]. These reference specimens shall be taken by cutting. Four pieces shall be cut from plate materials along the rolling directions. Table 1 Chemical composition of reference specimen (zinc plate) unit: % Zn Pb Fe ca Cu 98.5 min. 13 max. | 0.09 max. 0.40 max. 0.01 max The reference specimens shall be carefully cleaned immediately before testing. The dirt, oil and other impurities capable of influencing the test results shall be removed. In such a case, either of the following methods shall be used. a) Thoroughly clean the reference specimens with an appropriate organic solvent (the range of boiling point of hydrocarbon, 60 °C to 120 °C) using a clean, soft brush or an ultrasonic cleaning device. Carry out the cleaning in a vessel full of solvent at room temperature. After cleaning, rinse the reference specimens with fresh solvent and then dry them. b) If the similar results are obtained, other methods may be used in accordance with the agreement between the parties concerned with delivery. Weigh the reference specimens to the place of 1 mg. Protect the one surface of the reference specimens with a removable coating material, for example, an adhesive tape. 11.2.2 Arrangement of the reference specimens Position the four reference specimens in four different corners in the test chamber, with the uncoated surface upwards, and at an angle of 20° + 5°. The support for the reference specimens shall be made of, or coated with, inert materials such as plastics. The lower edge of the reference specimens shall be approximately level with the upper edge of the salt spray collector so as to be exposed as the same manner as the ordinary plane specimens. The test duration shall be 24 h.8 Z 2371 : 2000 11.2.3 Determination of decrement At the end of test, remove the coating, rinse the reference specimens with cold water and remove the salt deposit. Immerse them in the aqueous solution of chromic acid (300 g/!) prepared in such a manner that the chromic acid aqueous solution(*) conforming to the chemical composition given in Table 2 is diluted with the water of 7.1 b), at 25°C + 2 °C for 3 min, or immerse them in chromic acid aqueous solution (200 g/!) at 80 °C for 1 min, repeat the cleaning until the decrement change almost disappears and thoroughly remove the corrosion products. Rinse the reference specimens with warm water (40 °C + 5 °C), then dry them in a dryer at 105 °C, and furthermore cool them at room temperature. Weigh the mass of reference specimens to the place of 1 mg, and calculate the decrement of mass by the unit of g/m?. Note (*) Chrome oxide and aqueous solution of chromic acid are toxic, therefore care shall be thoroughly taken so as not to touch on skin or mucous membrane on handling. Table 2 Chemical composition of chrome (VI) oxide (chromic anhydride) Unit: % Aqueous| Chloride | Sulphate | Alkali earth and | Precipitated substance | Content solution (cn) (SO.)_ | alkali (sulphate) | by aqueous ammonia Limit | 0.005 max. | 0.005 max. 0.1 max. 0.03 max. 98.0 min. 11.2.4 Inspection of apparatus operation If the mass loss of each reference specimen at four positions is 40 g/m? + 12 g/m?, the apparatus shall be considered to operate satisfactorily. 11.3 CASS test 11.3.1 Reference specimens The reference specimens shall be as shown in 11.2.1 11.8.2 Arrangement of reference specimens The arrangement of reference specimens shall be as shown in 11.2.2 11.3.3 Determination of decrement The determination of decrement shall be as shown in 11.2.3 11.8.4 Inspection of apparatus operation If the mass loss of each reference specimens at four positions is 95 g/m? + 25 g/m’, the apparatus shall be considered to operate satisfactorily. 12 Start of test After the confirmation of 9, the spray is temporarily suspended, and a specimen is placed in the atomizing chamber to start the test. 13 Continuation of test The test shall be carried out continuously during the test period. However, it may be intermittently carried out subject to the agreement between the parties concerned with delivery.9 Z 2371 : 2000 When the test is interrupted to inspect and put in and take out of the specimen, the time of interruption shall be minimized by only stopping the atomization. 14 Duration of test The duration of the test shall be as specified according to the materials to be tested, product standards, ete. When not specified, it shall be subjected to the agreement between the parties concerned with delivery. The recommended exposure duration are 2 h, 6 h, 24 h, 48 h, 96 h, 168 h, 240 h, 480 h, 720 h and 1000 h. Informative reference: When the appearance of corrosion is observed, the test may be carried out until corrosion appears. 15 Treatment of specimen after test The specimen after the test shall be treated as follows: a) The speci dried for 0.5 h to 1.0 h. b). In order to remove the sodium chloride adhering to the surface of the specimen, the specimen shall be washed with water at ordinary temperature of 15 °C to 40 °C and dried immediately. r_and immediately Informative reference: The drying may be carried out by blowing the air of not exceeding 200 kPa in pressure at a distance of approxi- mately 300 mm. ©) In the case of removing corrosion products, they shall be removed by mechanical ‘Table 1 or Informative reference Table 2), or otherwise by combination of these 16 Evaluation method The method for evaluation of test results shall be in accordance with either of the following methods. However, other methods(”) may be applied subject to the agreement between the parties concerned with delivery. a) Area method The results shall be evaluated by the rating number method specified in Annex 1.(*) b) Mass method The change of mass of specimen before test and after removal i s by testing shall be examined and evaluated. For other methods, the method of appearance, record of change by microscopic photograph, elapsed time by the appearance of first sign of corrosion ete., are known. When the corrosion results are evaluated by the area method, a plane 17 Record The following items should preferably be recorded: a) Classification of test b) Name and type of test apparatus and system of atomizer.10 Z 2371 : 2000 ©) Shape and dimensions of specimens and members, or otherwise number or type of parts. d) Cleaning method of specimen before and after test e) Number of the specimens to be supplied for testing f) thod of specimen g) Existence and size of scratch, and device for scratchi h) Supporting angle of specimen. In the case of members, its supporting angle and method. i) Types of salt and water used for preparation of salt solution for testing i). Temperature around the specimen holder in the atomizing chamber k) Daily records of numerical. values obtained from each sampling container on the following items. 1) Volume (ml) of atomized solution sampled per hour for approximately 80 cm? 2) Salt concentration of sampled atomized solution and its measured value of density by hydrometer (25 °C) (in the case of neutral salt spray test) 3) pH of sampled atomized solution 1) When the test is carri intermi SP m) When the test is interrupted, its reason and duration of interruption n) Period of test the di ©) Specification of reference specimens used for the evaluation method of reproducibility of testing apparatus p) Whe q) Evaluation method and expression of results (including the results at intermediate inspection.) r) Photograph of specimen, if necessary.